反応 #640527

反応方程式

4-(1H-benzimidazol-2-yl)-furazan-3-yl-N-(2-cyanoethyl)-amine

4-(1H-Benzimidazol-2-yl)-furazan-3-yl-N-(2-cyanoethyl)-amine

LiAlH4

THF

THF

→

title compound

4-(1H-Benzimidazol-2-yl)-furazan-3-yl-N-(3-hydroxypropyl)-amine

反応条件

後処理

1. 1
   その他is quenched by careful addition of aqueous saturated solution of sodium sulphate
2. 2
   ろ過The suspension is filtered
3. 3
   その他the filtrate evaporated to dryness
4. 4
   その他Crystallization
5. 5
   workup.ADDITIONby addition of hexane

実験手順

A solution of 4-(1H-benzimidazol-2-yl)-furazan-3-yl-N-(2-cyanoethyl)-amine (0.272 g, 0.947 mmol, Example 6a) in THF (5 ml) is added dropwise at 0° C. to an efficiently stirred suspension of LiAlH4 (0.054 g, 1.42 mmol) in THF (5 ml). After stirring for 16 hours at room temperature the mixture is quenched by careful addition of aqueous saturated solution of sodium sulphate. The suspension is filtered and the filtrate evaporated to dryness. Crystallization by addition of hexane yields the title compound in pure form. 1H-NMR (400 MHz, d6-DMSO): 13.6 (s, 1H); 7.66 (m, 2H); 7.31 (m, 2H); 6.92 (t, 1H); 4.61 (m, 1H); 3.51 (m, 2H); 3.39 (m, 2H); 1.81 (m, 2H).

出典